HRID1285340
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 18 °C
PROCEDURE
实验过程
92 g of 2-cyano 3-(2,6-dichlorophenyl)propenoic acid (Tetrahedron Lett., 1975, p.3643-4) are put into 860 ml of methanol and 285 ml of a 10% sodium hydrogen carbonate solution. This is cooled to 18° C. and the necessary quantity of sodium borohydride is introduced over a two and one-half hour period. The mixture is left for 2 hours at ambient temperature, then concentrated and acidified by adding 1N hydrochloric acid until a pH of 2.3. The solution is then extracted with ether and the organic layer is washed with water, dried on magnesium sulphate, filtered and evaporated. 82.4 g of 2-cyano 3-(2,6-dichlorophenyl)propanoic acid are obtained.
WORKUP
后处理
- concentrationconcentrated
- additionby adding 1N hydrochloric acid until a pH of 2.3
- extractionThe solution is then extracted with ether
- washthe organic layer is washed with water
- customdried on magnesium sulphate
- filtrationfiltered
- customevaporated